CN109280959A - A method of semi-hydrated gypsum fiber is prepared by desulfurized gypsum - Google Patents
A method of semi-hydrated gypsum fiber is prepared by desulfurized gypsum Download PDFInfo
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- CN109280959A CN109280959A CN201710589297.3A CN201710589297A CN109280959A CN 109280959 A CN109280959 A CN 109280959A CN 201710589297 A CN201710589297 A CN 201710589297A CN 109280959 A CN109280959 A CN 109280959A
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- desulfurized gypsum
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A method of semi-hydrated gypsum fiber is prepared by desulfurized gypsum, the described method comprises the following steps: desulfurized gypsum is dried, removes free water therein；Desulfurized gypsum after drying is sieved, large granular impurity therein is removed；Desulfurized gypsum after screening is added in the hydrochloric acid containing magnesium chloride crystal modifier, is filtered after reacting a period of time at a certain temperature；The filter cake obtained after suction filtration is eluted with organic solvent；Filter cake after washing is dried to get semi-hydrated gypsum fiber is arrived.The draw ratio of the semi-hydrated gypsum fiber of the present processes preparation simplifies preparation process, reduces energy consumption, realize the cycling and reutilization of Industrial Solid Waste desulfurized gypsum up to 400.
Description
Technical field
This application involves but be not limited to inolrganic chemicals preparation field, be more particularly without limitation, to one kind by desulfurized gypsum
The method for preparing semi-hydrated gypsum fiber.
Background technique
Semi-hydrated gypsum fiber is the fibrous monocrystal of half-H 2 O calcium sulphate, is a kind of novel to have very high combination property
Inorganic material.Semi-hydrated gypsum fiber integrates the advantage of both reinforcing fiber and ultra-fine inorganic filler, can be used as strengthening and toughening
The height of agent or functional form filler for plastics, rubber, coating, paint, papermaking, pitch, friction and sealing material, covered electric cable is exhausted
In edge material.
The preparation method of gypsum fiber is mainly hydro-thermal method at present, and the temperature of hydro-thermal reaction is generally 105-150 DEG C or more
Height, pressure 200-500Kpa, the mode of filtering are generally filters pressing, and when filters pressing, temperature is generally not less than 100 DEG C, prepares
Gypsum fiber draw ratio is generally 50-200.The method is more demanding to technique, and energy consumption is larger.
Summary of the invention
It is the general introduction to the theme being described in detail herein below.This general introduction is not the protection model in order to limit claim
It encloses.
That this application provides a kind of process conditions is mild, energy consumption is lower prepares semi-hydrated gypsum fiber using desulfurized gypsum
Method.
Specifically, this application provides a kind of methods for preparing semi-hydrated gypsum fiber by desulfurized gypsum.
The method that semi-hydrated gypsum fiber is prepared by desulfurized gypsum provided herein, comprising the following steps:
It is dry: desulfurized gypsum being dried, free water therein is removed；
Screening: the desulfurized gypsum after drying is sieved, large granular impurity therein is removed；
Constant pressure hydro-thermal reaction: the desulfurized gypsum after screening is added in the hydrochloric acid containing magnesium chloride crystal modifier, in certain temperature
Degree filters after lower reaction a period of time；
Washing: the filter cake obtained after suction filtration is eluted with organic solvent；
It is dry: the filter cake after washing to be dried to get semi-hydrated gypsum fiber is arrived.
In presently filed embodiment, described desulfurized gypsum is dried can be by desulfurized gypsum at 40-50 DEG C
Lower dry 4-6h.
In presently filed embodiment, the screening can be that 100-300 mesh is sieved.
In presently filed embodiment, the concentration of the hydrochloric acid can be 1mol/L.
In presently filed embodiment, the quality of the magnesium chloride can be the 0.5% of hydrochloric acid quality.
In presently filed embodiment, the mass ratio of the desulfurized gypsum after the hydrochloric acid and screening can be (8-11):
1。
In presently filed embodiment, the reaction temperature of the constant pressure hydro-thermal reaction can be 90-97 DEG C, the reaction time
It can be 5-8h.
In presently filed embodiment, the organic solvent can be dehydrated alcohol.
In presently filed embodiment, the drying temperature of the filter cake can be 90-97 DEG C, and drying time can be 3-
10h。
The preparation of semi-hydrated gypsum fiber can be realized under conditions of normal pressure, lower temperature by the present processes.Though
So without wishing to be bound by theory, but present inventor speculates that reason may be: CaSO4·2H2O has by Ca2+With
SO4 2-The sheath of formation layer structure staggered with water molecule layer；When normal pressure acidization makes its transformation tissue culture, hot solution meeting
It is immersed in interlayer, strong heat is generated to it and transmits and is evenly heated it, CaSO4·2H2O occurs to dissolve and is ionized into Ca2+
And SO4 2-, work as Ca2+And SO4 2-Concentration when being greater than transformation tissue culture product equilbrium solubility at such a temperature, converted product is mutually brilliant
Core starts to be precipitated, the Ca in solution2+And SO4 2-It is generated on nucleus and adsorbs and start to grow, form transformation tissue culture product；Turn crystalline substance
The Mg of agent2+SO can be adsorbed in4 2-On the crystal face (200), (400) and (020) of dense distribution, inhibit CaSO4·0.5H2O crystal
To lateral growth, to make CaSO4·0.5H2O grows along c-axis and ultimately forms the big crystal of draw ratio (referring to as shown in Figure 1
Calcium sulfate crystal pattern).
The draw ratio of the semi-hydrated gypsum fiber of the present processes preparation simplifies preparation process, reduces energy up to 400
Consumption, realizes the cycling and reutilization of Industrial Solid Waste desulfurized gypsum.
Other features and advantage will illustrate in the following description, also, partly become from specification
It obtains it is clear that being understood and implementing the application.The purpose of the application and other advantages can be by specifications, right
Specifically noted structure is achieved and obtained in claim and attached drawing.
Detailed description of the invention
Attached drawing is used to provide to further understand technical scheme, and constitutes part of specification, with this
The embodiment of application is used to explain the technical solution of the application together, does not constitute the limitation to technical scheme.
Fig. 1 is the crystal pattern of calcium sulfate.
Fig. 2 is the XRD diagram of desulfurized gypsum raw material.
Fig. 3 a)-b) it is SEM figure of the desulfurized gypsum raw material under different amplification.
Fig. 4 is the XRD diagram of semi-hydrated gypsum fiber prepared by the embodiment of the present application 1.
Fig. 5 a)-b) it is SEM figure of the semi-hydrated gypsum fiber of the preparation of the embodiment of the present application 1 under different amplification.
Specific embodiment
For the purposes, technical schemes and advantages of the application are more clearly understood, below in conjunction with attached drawing to the application
Embodiment be described in detail.It should be noted that in the absence of conflict, in the embodiment and embodiment in the application
Feature can mutual any combination.
Raw materials and reagents used in following embodiment are unless otherwise instructed ordinary commercial products.
Embodiment 1
The desulfurized gypsum for choosing Zhongweiof Ningxia, northwest China power plant, dry 4h, crosses 200 meshes, it is thin to obtain desulfurized gypsum at 40 DEG C
1g desulfurized gypsum fine powder is added to the salt for the 1mol/L (density is about 1.01g/ml) that 8ml contains 0.5wt% magnesium chloride by powder
In acid solution, ultrasonic 5min keeps desulfurized gypsum evenly dispersed, after reacting 7h at 93 DEG C, carries out rapid filtration under suction, and with anhydrous
Ethyl alcohol elutes filter cake, and the filter cake after elution is placed in in 93 DEG C of drying box dry 5h to get semi-hydrated gypsum fiber is arrived.
Embodiment 2
The desulfurized gypsum for choosing Zhongweiof Ningxia, northwest China power plant, dry 5h, crosses 230 meshes, it is thin to obtain desulfurized gypsum at 45 DEG C
3g desulfurized gypsum fine powder is added in the hydrochloric acid solution for the 1mol/L that 25ml contains 0.5wt% magnesium chloride, ultrasonic 8min by powder,
Keep desulfurized gypsum evenly dispersed, after reacting 6h at 95 DEG C, carry out rapid filtration under suction, and eluted to filter cake with dehydrated alcohol,
Filter cake after elution is placed in in 95 DEG C of drying box dry 6h to get semi-hydrated gypsum fiber is arrived.
Embodiment 3
The desulfurized gypsum for choosing Zhongweiof Ningxia, northwest China power plant, dry 6h, crosses 230 meshes, it is thin to obtain desulfurized gypsum at 50 DEG C
5g desulfurized gypsum fine powder is added in the hydrochloric acid solution for the 1mol/L that 50ml contains 0.5wt% magnesium chloride, ultrasonic 8min by powder,
Keep desulfurized gypsum evenly dispersed, after reacting 8h at 97 DEG C, carry out rapid filtration under suction, and eluted to filter cake with dehydrated alcohol,
Filter cake after elution is placed in in 97 DEG C of drying box dry 8h to get semi-hydrated gypsum fiber is arrived.
Test case
1, desulfurized gypsum raw material and the application are tested using SHIMADZU XRD-7000 type X-ray diffraction analysis instrument respectively
The XRD spectrum of semi-hydrated gypsum fiber prepared by embodiment 1.
Test condition: Cu target K alpha ray source, tube voltage 40kV, tube current 30mA, sweep speed are 2 °/min.Test
As a result see Fig. 2 and Fig. 4.
The variation of comparison diagram 2 and Fig. 4, XRD characteristic peak position illustrate desulfurized gypsum through side described in the embodiment of the present application 1
After method conversion, object mutually becomes half-H 2 O calcium sulphate from calcium sulphate dihydrate.
2, it tests desulfurized gypsum raw material respectively using S-4800 field emission scanning electron microscope (FESEM) and the application is real
Apply SEM figure of the semi-hydrated gypsum fiber of the preparation of example 1 under different amplification.
Test condition: acceleration voltage 15kV.Test result is see Fig. 3 and Fig. 5.
After comparison diagram 3 and Fig. 5 can be seen that desulfurized gypsum method conversion described in the embodiment of the present application 1, microscopic appearance
Threadiness is changed by large grained.
The length of the semi-hydrated gypsum fiber of embodiment 1-3 preparation is about 300-350 μm, diameter is about 0.8 μm, and draw ratio is about
It is 400.
Although embodiment disclosed by the application is as above, the content only for ease of understanding the application and use
Embodiment is not limited to the application.Technical staff in any the application fields, is taken off not departing from the application
Under the premise of the spirit and scope of dew, any modification and variation, but the application can be carried out in the form and details of implementation
Scope of patent protection, still should be subject to the scope of the claims as defined in the appended claims.
Claims (9)
1. a kind of method for preparing semi-hydrated gypsum fiber by desulfurized gypsum, the described method comprises the following steps:
It is dry: desulfurized gypsum being dried, free water therein is removed；
Screening: the desulfurized gypsum after drying is sieved, large granular impurity therein is removed；
Constant pressure hydro-thermal reaction: the desulfurized gypsum after screening is added in the hydrochloric acid containing magnesium chloride crystal modifier, at a certain temperature
It is filtered after reaction a period of time；
Washing: the filter cake obtained after suction filtration is washed with organic solvent；
It is dry: the filter cake after washing to be dried to get semi-hydrated gypsum fiber is arrived.
2. according to the method described in claim 1, wherein, it is described by desulfurized gypsum be dried for by desulfurized gypsum in 40-50
Dry 4-6h at DEG C.
3. according to the method described in claim 1, wherein, the screening was that 100-300 mesh is sieved.
4. according to the method described in claim 1, wherein, the concentration of the hydrochloric acid is 1mol/L.
5. according to the method described in claim 1, wherein, the quality of the magnesium chloride is the 0.5% of hydrochloric acid quality.
6. method according to claim 4 or 5, wherein the mass ratio of the desulfurized gypsum after the hydrochloric acid and screening is (8-
11):1。
7. the reaction temperature of the constant pressure hydro-thermal reaction is 90-97 DEG C according to the method described in claim 1, wherein, when reaction
Between be 5-8h.
8. according to the method described in claim 1, wherein, the organic solvent is dehydrated alcohol.
9. according to the method described in claim 1, wherein, the drying temperature of the filter cake is 90-97 DEG C, drying time 3-
10h。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710589297.3A CN109280959A (en) | 2017-07-19 | 2017-07-19 | A method of semi-hydrated gypsum fiber is prepared by desulfurized gypsum |
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| CN201710589297.3A CN109280959A (en) | 2017-07-19 | 2017-07-19 | A method of semi-hydrated gypsum fiber is prepared by desulfurized gypsum |
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